Some standard content:
National Standard of the People's Republic of China
Food additives
Saccharin sodium
UDC 661.73
GB 4578--84
This standard applies to saccharin sodium produced by chemical synthesis with phthalic anhydride or toluene as raw materials, as a food sweetener. Structural formula:
NNa*2H,0
Molecular formula: C,H,O3NSNa·2H,O
Molecular weight: 241.19
1 Technical requirements
1.1 Appearance
Colorless crystals or slightly white crystalline powder, odorless or slightly fragrant, strong sweet taste with bitterness. 1.2
The quality specifications of saccharin sodium shall meet the following requirements: Index name
Content (based on dry product), %
Loss on drying, %
Ammonium salt (based on NH), %
Heavy metal (based on Pb), %
Arsenic salt (based on As), %
Test method
2.1 Identification
2.1.1 Reagents and solutions
2.1.1.1 Resorcinol (HGB3374-60) Issued by the State Bureau of Standards on July 13, 1984
Implemented on April 1, 1985
2.1.1.2 Sulfuric acid (GB 625-77)
GB 4578--84bZxz.net
2.1.1.3 Sodium hydroxide (GB629-77): 4% solution, 2.1.1.4 Hydrochloric acid (GB 622~77): 10% solution. 2.1.2 Instruments and equipment
2.1.2.1 General laboratory instruments.
2.1.3 Operation steps
2.1.3.1 Take about 20 mg of the sample, add about 40 mg of resorcinol, mix and add 10 drops of sulfuric acid, heat with a low fire until it turns dark green, cool, add 10 ml of water and excess sodium hydroxide solution, and a green fluorescent solution will be formed. 2.1.3.2 Take a platinum wire, wet it with hydrochloric acid, dip it in the sample, and burn it in a colorless flame. The flame will Bright yellow. 2.1.4 Melting point determination
2.1.4.1 Instruments and equipment
According to the melting point determination method of the 1977 edition of the Pharmacopoeia of the People's Republic of China. 2.1.4.2 Take about 0.3g of the sample, add 5ml of water to dissolve it, add 1ml of dilute hydrochloric acid, and crystals will precipitate. Filter it, wash the filter residue with water, and dry it at 105℃. Its melting point should be 226~230℃. 2.2 Determination of saccharin sodium content
2.2.1 Reagents and solutions
2.2.1.1 Glacial acetic acid (GB 676-78), 2.2.1.2 Acetic anhydride (GB 677--78) 3
2.2.1.3 Crystal violet indicator solution: 0.5% acetic acid solution; 2.2.1.4 Anhydrous acetic acid: Take an appropriate amount of glacial acetic acid, and add 5.22ml of acetic anhydride to 1g of water according to the water content. 5 Perchloric acid (GB623-77): 0.1N standard solution, prepared according to GB601-77 "Preparation Method for Standard Solution of Chemical Reagents".
2.2 .2 Instruments
General laboratory instruments and automatic burette (25ml). 2.2.3 Determination procedures
Take 0.3g of the sample after the drying loss determination, weigh it to 0.0002g, add 20ml of acetic acid and 5ml of acetic anhydride, dissolve it, add 2 drops of crystal violet indicator solution, and titrate it with 0.1N perfluoric acid standard solution until it turns blue-green. 2.2.4 Calculation
The percentage content of saccharin sodium (X) is calculated according to formula (1): X = N×V×0.2052
Wherein: N-
Equivalent concentration of perchloric acid standard solution,
-Volume of perchloric acid standard solution consumed, ml,-Sample mass, g,
-Number of grams of 1 mg equivalent saccharin sodium.
2.3 Determination of loss on drying
2.3.1 Apparatus and equipment
General laboratory instruments and agate mortar (d50mm) 2.3. 1.1
2.3.1.2 Electric constant temperature drying oven (room temperature to 200℃) or infrared drying oven. 2.3.2 Determination procedure
Take 0.5g of the ground sample, weigh it to 0.0002g, dry it at 105℃ to constant weight, or dry it in an infrared drying oven for two hours. 2.3.3 Calculation
The percentage loss on drying (X) is calculated according to formula (2): 418
Where: m
GB 4578~-84
-mass of the sample plus the weighing bottle before drying, g, f-mass of the sample plus the weighing bottle after drying, g,
-mass of the sample, g.
2.4 Determination of ammonium salt
2.4.1 Reagents and solutions
ml-m2 × 100
2.4.1.1 Alkaline potassium mercuric iodide solution: Take 10g potassium iodide (GB1272--77) and 13.5g mercuric iodide (HG3-1067-77), dissolve in water and dilute to 100ml, mix with an equal volume of 25% sodium hydroxide solution before use. 2.4.1.2 Dilute sulfuric acid: Take 5.7ml sulfuric acid (GB625-77), dilute to 100ml with water. 2.4.1.3 Potassium permanganate solution: Take 0.33g potassium permanganate (GB643-77), add 100ml water, boil for 15min, seal tightly, let stand for more than 2 days, filter with a vertical fused glass filter, and shake well. 2.4.1.4 Ammonia-free water: Take 1000ml of distilled water, add 1ml of dilute sulfuric acid and 1ml of potassium permanganate solution, distill, and obtain. Take 50ml and add 1ml of alkaline potassium mercuric iodide solution. No color should be developed. 2.4.1.5 Ammonium standard solution: Prepare according to GB602-77 "Preparation Method of Standard Solution of Chemical Reagent Impurities", 1ml contains 0.1mg NHI.
2.4.2 Instruments
2.4.2.1 General laboratory instruments and Nessler colorimetric tube (50ml). 2.4.3 Determination procedures
Take 0.4g of the sample, weigh to 0.01g, add 20ml of hydrogen-free water, dissolve, add 1ml of alkaline potassium mercuric iodide solution, shake well, and let stand for 5min. If color is developed, compare it with the color developed by 0.1ml of standard ammonium chloride solution, 19.9ml of ammonia-free water and 1ml of alkaline potassium mercuric iodide solution, and it shall not be darker.
2.5 Determination of arsenic salts
2.5.1 Reagents and solutions
2.5.1.1 Anhydrous sodium carbonate (GB639-77) 2.5.1.2 Hydrochloric acid (GB 622-77)
2.5.1.3 Potassium iodide (GB1272--77): 15% solution, 2.5.1.4 Stannous chloride (GB638-78): 40% hydrochloric acid solution, prepared according to GB603-77 "Chemical Reagent Preparations and Products Preparation Methods",
2.5.1.5 Arsenic-free metallic zinc (GB2304-80), 2.5.1.6 Lead acetate cotton: prepared according to GB603-77, 2.5.1.7
Mercuric bromide test paper: prepared according to GB603-77: 2.5.1.8 Monel standard solution: prepared according to GB602-77 "Chemical Reagent Impurity Standard Solution Preparation Method", diluted 100 times, the obtained solution contains 1ug of monument per ml.
2.5.2 Instruments and Devices
Arsenic determination device, according to the provisions of the "Arsenic Salt Inspection Method" of the 1977 edition of the "Pharmacopoeia of the People's Republic of China". 2.5.3 Determination Procedures
Take 1g of anhydrous sodium carbonate and spread it on the bottom and around the crucible, then take 1g of the sample, weigh it to 0.1g, place it on the sodium carbonate, and moisten it with a small amount of water. 1 After drying, first use an electric furnace to carbonize, and then burn at about 600℃ to completely carbonize, cool, add hydrochloric acid to neutralize and acidify, add 23ml of water to dissolve, and transfer to a 100ml conical flask, add 5ml of potassium iodide solution and 5 drops of acidic stannous chloride solution, after leaving it at room temperature for 10 minutes, add 1.5g of metal-free zinc, immediately install the arsenic determination tube filled with lead acetate cotton and mercuric bromide test paper, leave it at 25-40℃ for 1h, take out the mercuric bromide test paper, and compare the generated spot with the standard arsenic spot obtained by accurately measuring 2ml of standard arsenic solution, adding 5ml of hydrochloric acid, 21ml of water, 5ml of potassium iodide solution, 5 drops of acidic stannous chloride solution, and treating it in the same way as above. It shall not be darker. 419
2.6 Determination of heavy metals
2.6.1 Reagents and solutions
GB 4578--84
2.6.1.1 Hydrochloric acid (GB 622-77): 1N solution2.6.1.2 Glacial acetic acid (GB 676-78): 6% solution;2.6.1.3 Saturated aqueous solution of hydrogen sulfide: prepared according to GB603-77 (prepared and used immediately)2.6.1.4 Lead standard solution: Prepare according to GB602-77 and dilute 10 times. 1 ml of solution contains 10 g of lead. 2.6.2 Determination procedures
Take 2 g of the sample (weighed to 0.1 g) and place it in a beaker. Add 48 ml of water. After dissolving, add 2 ml of 1N hydrochloric acid solution, stir evenly, and rub the wall of the cup with a glass rod until it begins to crystallize. After standing for 1 hour, filter, discard the initial filtrate 10 ml, take the remaining filtrate 25 ml as A, take another 1 ml of standard lead solution and dilute it to 25 ml with water as B, add 1 ml of 6% acetic acid and 10 ml of saturated aqueous solution of hydrogen sulfide to A and B respectively, place them in a dark place for 10 minutes, then take them out for comparison. A shall not be darker than B.
3 Acceptance rules
3.1 This product shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all products shipped meet the requirements of this standard. Each batch of products shipped shall be accompanied by a quality certificate. 3.2 The user can verify whether the received products meet the requirements of this standard according to the inspection rules and test methods specified in this standard. 3.3 Sampling method: Samples should be selected from 10% of the barrels in each batch. In the case of small batches, no less than 3 barrels should be selected. Samples of no less than 100g should be taken out, and the selected samples should be quickly mixed. Three times the amount required for testing should be taken for testing and analysis. 3.4 If one of the indicators in the inspection does not meet the requirements of this standard, samples should be selected from the packaging of twice the amount for verification. If the result of the re-inspection of the product does not meet the requirements of this standard even if only one indicator does not meet the requirements of this standard, the entire batch cannot be accepted. 3.5 The weight of each batch shall not exceed the actual batch output of the manufacturer. 3.6 If the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the Food Hygiene Law of the People's Republic of China (Trial Implementation). 4 Packaging, marking, storage and transportation
4.1 Saccharin sodium is divided into 9 kinds of packaging: 50kg, 25kg, 0.5kg and 10g. 4.250kg and 25kg are packed in barrels. The products are first packed in polyethylene bags for food, sealed, covered with kraft paper bags and then stored in wooden barrels or cardboard barrels.
0.5kg and 10g are packed in polyethylene bags for food. Each certain quantity is packed in a corrugated box. 4.3'Transportation must be covered to avoid sun, rain, heat and impact. Be careful when handling and loading and unloading. 4.4 Store in a cool and dry warehouse. The pad should be more than 100mm above the ground to avoid heat and moisture. 4.5 This product must not be mixed, transported or stacked with toxic substances during storage and transportation. The outer packaging should be marked with food additives and standard numbers. Additional remarks:
This standard was proposed by the Ministry of Health and the Medical Administration of the People's Republic of China, and is under the jurisdiction of the Food Hygiene Supervision and Inspection Institute of the Ministry of Health and the Medical Administration Week.
This standard was drafted by the Shanghai Municipal Health and Epidemic Prevention Station and the Shanghai Sixth Pharmaceutical Factory. The main drafters of this standard are Yuan Yicheng and Tang Jianzhong. 420
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